化工社
首页MCP工作台Skills
首页工作台通知我的
llms.txt · MCP 指南隐私政策 · 服务条款 · 支持v1.8.0
  1. 首页
  2. /反应

三氟乙酸 → HCID 21191156,化合物

HRID 1069088
笔记
打印预览

反应方程式

HRID 1069088 反应方程式
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH2:18][CH2:19][NH:20]C(OC(C)(C)C)=O)[CH:12]=2)[CH:8]=[CH:9][CH:10]=1)=[O:4].FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH2:18][CH2:19][NH2:20])[CH:12]=2)[CH:8]=[CH:9][CH:10]=1)=[O:4]
参与物实验过程后处理来源与证据反应笔记

参与物

4

反应物 2

HCID 6422三氟乙酸2 次HCID 54336416HCID 54336416,化合物

产物 1

HCID 21191156HCID 21191156,化合物收率 98.5%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

The methyl-3′-[2-[[(tert-butoxy)carbonyl]amino]ethoxy]-[1,1′-biphenyl]-3-carboxylate (659 mg) was dissolved in methylene chloride (25 mL) and trifluoroacetic acid (2.5 mL) was added. The mixture was stirred at room temperature for 6 h, additional trifluoroacetic acid (1.0 mL) was added and the mixture was stirred overnight. The mixture was concentrated and partitioned between saturated aqueous sodium bicarbonate and ethyl acetate. The organic layer was separated, dried over sodium sulfate, filtered and concentrated to give the crude product. This residue was partitioned between 1:1 hexane: ethyl acetate and 1 N aqueous HCl. The aqueous layer was separated, washed with 1:1 hexane: ethyl acetate and made basic by addition of solid sodium bicarbonate. The mixture was extracted twice with ethyl acetate, and the combined organic extracts were dried over sodium sulfate, filtered and concentrated to afford the title compound (474 mg) as a colorless oil. Electrospray MS (positive ion): (M+H) 272.0.

后处理

  1. stirringthe mixture was stirred overnight
  2. concentrationThe mixture was concentrated
  3. custompartitioned between saturated aqueous sodium bicarbonate and ethyl acetate
  4. customThe organic layer was separated
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give the crude product
  9. customThis residue was partitioned between 1:1 hexane
  10. customThe aqueous layer was separated
  11. washwashed with 1:1 hexane
  12. additionethyl acetate and made basic by addition of solid sodium bicarbonate
  13. extractionThe mixture was extracted twice with ethyl acetate
  14. dry with materialthe combined organic extracts were dried over sodium sulfate
  15. filtrationfiltered
  16. concentrationconcentrated

来源与证据

ORD记录
ord-66f9ec29f64b4aac90bd651018e8bb33
来源数据集
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
专利号
US06251925B1

反应笔记

加载中…

本页导航参与物实验过程后处理来源与证据反应笔记